CN113249547A - Smelting method for refining inclusions in H13 hot work die steel - Google Patents
Smelting method for refining inclusions in H13 hot work die steel Download PDFInfo
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Abstract
A smelting method for refining inclusions in H13 hot work die steel, in particular to a smelting method for refining inclusions in H13 hot work die steel. Feeding composite powder of Al-Si powder wrapped by iron sheet into melt by a method of small amount supply in different areasA large amount of spherical nano-grade Al is formed in the molten steel2O3‑SiO2And (3) impurities are similar, a flow field is formed in the melt by adopting a bottom blowing argon mode, and finally, a high-grade high-quality H13 hot-work die steel ingot with uniform structure and excellent performance is obtained (the grade of the impurities A + B + C + D + DS is less than or equal to 2.5). The method has the advantages of short casting period, low cost, mass production and little restriction on product complexity, greatly improves the strength and plasticity of metal materials, greatly improves the tensile strength and toughness of the prepared H13 hot-work die steel ingot with nano-sized inclusions, and meets the performance requirements of North America NADCA on high-grade die steel.
Description
Technical Field
The invention belongs to the technical field of refining inclusions in die steel, and particularly relates to a smelting method for refining inclusions in H13 hot work die steel.
Background
The 4Cr5MoSiV1 (H13) hot die steel is used as chromium air-cooling hardening type hot die steel, is widely used as a material of a hot forging die, a hot extrusion die and a large-sized die-casting die, can be used for manufacturing a plastic die on some occasions, and is one of hot die steel types which are used in the world at present and are the largest in dosage. The H13 hot work die steel is generally very harsh in industrial production, and is often required to withstand the effects of high temperature, high pressure, strong abrasion, thermal fatigue, stress corrosion and the like during working, and also to withstand the repeated thermal shock and mechanical shock of the high temperature alloy molten metal, which require the H13 hot work die steel to have high hardness, corrosion resistance, excellent thermal fatigue resistance and the like.
In H13 hot work die steel mainly suffering from fatigue fracture, the inclusions present in the structure thereof have a great influence on the service life thereof, and in particular, some brittle inclusions and irregular inclusions, etc. present in the steel matrix, tend to form strong stress concentrations. Experimental studies by Tridello et al show that the size of inclusions in H13 hot die steel has a great influence on the fatigue limit of steel in the use process, and through the research on the influence of the size of inclusions in H13 hot die steel on the fatigue limit of steel, the fatigue limit of H13 hot die steel is reduced by 21% when the size of the inclusions in H13 steel is maximum 31um [ A. Tridello et al, VHCF strength H gradient in large H13 steel special cases]. Procedia Structural Integrity, 2016, 2 : 1117-1124.]. Liujianhua et al analyzed the distribution of inclusions in H13 hot work die steel ingot and found that the types of inclusions in the ingot are mainly near-spherical CaO-Al2O3-SiO2Inclusions, irregularly shaped MgO-Al2O3The inclusions, massive TiN-VN inclusions, as well as strip-shaped VC-CrC-MoC inclusions and a small amount of CaS-MnS inclusions distributed along grain boundaries and the like are researched and found to be large-sized strip-shaped CaO-Al inclusions2O3-SiO2The impact of Inclusions on the toughness of H13 hot-work die Steel [ Hao Wang et al Formation and Evolution of Non-Metallic Inclusions in Calcium Treatment H13 Steel reducing Electroslag Replacing Process [ J]. ISIJ International, 2019, 59(5) : 828-838.]Therefore, it is necessary to control the size of the alloy during melting. In addition, the research also finds that the Steel ingot has a small quantity of inclusions near the center of the head, a large quantity of inclusions at the middle part and the tail part, a great difference between the total oxygen quantity of the center part and the head part structure, nonuniform distribution of the inclusions in the structure and a large quantity of large-size inclusions [ Jianan-hua Liu et al, inclusion variation Variations of Hot Working Die Steel H13 in Refining Process [ J-hu Liu et al].Journal of Iron and Steel Research International,2012,19(11):1-7.]. The experimental study of the H13 hot work die steel under argon protection and electroslag remelting in the atmosphere by Huangyu et Al and the analysis of inclusions in the prepared steel ingot show that the H13 hot work die steel produced by the protective atmosphere electroslag remelting process has low oxygen content, the mass fraction of the H13 hot work die steel is only 0.0015%, and oxide inclusions are mainly MgO-Al2O3-SiO2And inclusions, wherein small-size D-type oxide inclusions with the size of 1-3 mu m account for 62.5% of total inclusions, and in comparison, the mass fraction of oxygen in H13 hot work die steel which is not prepared by adopting a protective atmosphere is higher and is 0.0024% [ Huangyu, Xiexi, Kongguang, display, Zhandong, Severe, and strict-definition-faithful ] H13 steel forms Mg-Al-O series inclusions and controls [ J-Al-O series inclusions]Steel 2017,52(06):34-39.]. H13 hot work die steel imported from abroad contains a large amount of fine Al2O3-SiO2The sizes of the inclusions are less than 1.5um, and a large amount of nano-scale inclusions exist, and researches show that nano-scale Al in the tissues is in dispersed distribution2O3-SiO2The inclusions have no influence on the fatigue performance of the H13 hot work die steel basically; at present, the domestic H13 hot work die steel is mainly produced by adopting an electroslag remelting process and vacuum meltingSmelting process, however, the D-type Al in H13 hot work die steel obtained by electroslag remelting or vacuum smelting process2O3-SiO2The majority of the inclusions are concentrated in 2-3 um and there is a small amount of Al2O3-SiO2The size of the inclusions can reach 5 mu m and still be micron-sized inclusions, the grade A + B + C + D + DS of the inclusions is less than or equal to 4, the micron-sized inclusions still have great influence on the fatigue performance of the H13 hot work die steel, and the inclusions are difficult to use in some environments with very strict working requirements. In addition, the shape of the inclusion in the H13 hot-work die steel structure has great influence on the performance of the die steel, the shape of the inclusion is defined by the aspect ratio of the inclusion, the aspect ratio of the inclusion is the ratio of the longest axis passing through the centroid of the inclusion to the short axis perpendicular to the centroid of the inclusion, the smaller the aspect ratio is, the closer the shape of the inclusion is to the spherical shape, the larger the aspect ratio is, the closer the inclusion is to the long shape, and the test shows that the long shape of the long CaO-Al alloy is2O3-SiO2Inclusions greatly reduce the toughness of the H13 hot work die steel. Al in H13 hot work die steel2O3-SiO2The inclusions account for the majority of the total inclusions, and therefore how to hot work H13 into die steel such as CaO-Al2O3-SiO2Further controlling the size of the inclusions to obtain nanoscale Al2O3-SiO2H13 hot work die steel with more inclusions and only containing a small amount of micron-sized inclusions; at present, the grade A + B + C + D + DS of the inclusions in the high-quality H13 hot-work die steel is less than or equal to 4.5 according to the North American NADCA die-casting association regulation, the grade A + B + C + D + DS of the inclusions in the high-quality H13 hot-work die steel is less than or equal to 3, the size of the inclusions has obvious influence on the performance of the H13 hot-work die steel, and therefore, how to reduce the Al content in the H13 steel2O3-SiO2The aspect ratio of the inclusions is tied up, and the size of the inclusions in the steel is reduced so as to improve the performance of the H13 hot work die steel, and the method is one of the research focuses of the smelting process of the H13 hot work die steel.
Disclosure of Invention
The invention aims to provide a smelting method for refining inclusions to be nano-scale in H13 hot-work die steel, which feeds an iron sheet-coated Al-Si compound into molten steel in a multi-point area micro-supply modePreparing a great amount of nano-scale and a very small amount of micron-scale Al by matching the powder body with a bottom blowing argon method2O3-SiO2The inclusion-like H13 hot-work die steel ingot with uniform distribution has the inclusion grade A + B + C + D + DS less than or equal to 2.5, thereby solving the problem that large-size Al exists in the ingot casting structure of the H13 hot-work die steel in the casting process2O3-SiO2The problem of more inclusions is solved, and the performance of H13 hot work die steel cast ingots is greatly improved;
according to the first aspect of the invention, the nano-phase inclusion is added into the molten steel in a mode of 'multi-point regional micro supply' to form elements Al and Si, Al-Si composite powder is fed into the molten steel from a plurality of regions simultaneously, the extremely fine Al-Si powder is combined with O in the molten steel to form a large amount of nano-scale and extremely small amount of micron-scale nano-phase, the powder is fed into the plurality of regions simultaneously, so that the nano-phase can be uniformly formed and dispersed in the molten steel, the nano-phase is prevented from growing and aggregating by combining with low argon blowing, the size of D-type inclusion in H13 hot-work die steel is reduced, and finally, a high-grade high-quality H13 hot-work die steel ingot with uniform tissue and excellent performance is obtained.
According to the second aspect of the invention, a smelting method for refining inclusions in H13 hot work die steel is provided, a flow field and a force field are formed in molten steel in a bottom blowing argon mode, Al-Si powder wrapped by an iron sheet is combined with oxygen in the molten steel after the iron sheet is melted to form a large number of nano phases, and the formed nano phases are dispersed and distributed in the molten steel under the action of the flow field and the force field, so that the nano phases are prevented from being aggregated and grown up, and the method comprises the following steps:
step 1: preparing chemical materials according to predetermined weight percentages of the element components, and placing the metal materials according to the placing principle that the middle of a placing area is high, the periphery of the placing area is low, the placing of the lower half part is compact, and the placing of the upper half part is loose;
step 2: preparing H13 hot die steel liquid and alloying by adopting a smelting mode of smelting and heating in a vacuum arc furnace;
and step 3: after the LF refining operation is finished, feeding the composite powder with the Al-Si powder wrapped by the iron sheet into the molten steel in a multipoint regional micro-supply mode;
and 4, step 4: feeding powder into the melt, then measuring the oxygen concentration, and carrying out VD vacuum refining operation when the concentration of free oxygen is about 10 ppm;
and 5: forming a flow field in the melt by bottom blowing argon into the melt, so that powder wrapped in the molten iron sheet is uniformly distributed in the molten steel;
step 6: and pouring the prepared H13 hot-work die steel liquid into a casting mold to be uniformly solidified, and analyzing the size, the form, the components, the quantity, the distribution and the like of inclusions in the ingot casting structure.
Further, the die steel grade comprises the following chemical components in percentage by weight: 0.32-0.45 wt.% of C, 0.80-1.20 wt.% of Si, 0.20-0.50 wt.% of Mn, 0.80-1.20 wt.% of V, 4.75-5.50 wt.% of Cr, 1.10-1.75 wt.% of Mo, less than or equal to 0.03 wt.% of P, less than or equal to 0.03 wt.% of S, and the balance of Fe.
Further, in the step 2, by using the electric arc furnace smelting heating mode, before tapping, a high-level bunker can be adopted to add 400kg of lime and 10-30kg of carbon powder into the molten pool for pre-deoxidation and slag tapping, and tapping can be performed after the operation is finished. The step 2 of preparing molten steel and alloying by using the electric arc furnace smelting heating mode comprises the following steps: and heating and melting the alloy into molten steel by using a vacuum melting heating mode, carrying out alloying operation after the molten steel is completely melted, and then overheating and heating to 50-100 ℃ until the molten steel surface is stable.
Furthermore, in the wire feeding process adopting the iron sheet to wrap the Al-Si powder in the step 3, the composite powder wrapped by the iron sheet is required to be melted in the deep part of the molten steel, so that the powder feeding depth is ensured to be more than 300 mm; in order to ensure that the iron sheet can be melted in time to release the internal Al-Si powder when a wire made of Al-Si powder wrapped by the iron sheet is fed to the bottom of molten steel, and the powder can be fully contacted with the molten steel in the molten steel, the thickness of the iron sheet needs to be controlled to be about 0.1-0.2 mm, so that the melting time of the iron sheet is 1-1.5 s, and the efficiency is improved.
Furthermore, the feeding of the Al-Si composite powder in the step 3 is mainly determined by the purpose, and the feeding of the composite powder with the Al-Si powder wrapped by the iron sheet is mainly to improve the internal quality in the molten steel and takeInstead of the traditional smelting mode of directly smelting the aluminum blocks and the silicon wafers together with other metal materials, the composite powder of Al-Si powder wrapped by iron sheets is simultaneously fed into different areas of molten steel by adopting a multipoint area micro-supply method, so that a large amount of nano-scale inclusions are formed in the molten steel, and particularly Al is enabled to be formed2O3-SiO2The inclusion-like substances do not exist in the steel material in the form of a strip, but exist in the form of spherical nano-scale inclusion, thereby improving the internal quality of molten steel.
Further, in the step 5, argon is blown into the molten steel to form bubbles moving from bottom to top under the action of buoyancy, and the bubbles can draw the molten steel and enable the molten steel to flow from bottom to top in the process of floating in the molten steel; when the bubbles float to the liquid level, the bubbles start to move to the horizontal direction and move to the container wall, and the bubbles flow back and forth in the molten steel to form a circulation; in the process, the inclusions and oxides with super-large sizes are dragged to float to top slag to be removed when bubbles float; meanwhile, bubbles originally existing in the molten steel are fused and taken out of the molten steel, so that the defects of shrinkage cavity and looseness possibly existing in the subsequent solidification are overcome; in addition, argon is introduced to form a flow field and a force field in the molten steel, so that the powder fed in the step 3 can be uniformly distributed in the molten steel and is not easy to gather to form large-size Al2O3-SiO2And (4) inclusion-like substances.
The invention provides a smelting method for refining inclusions in H13 hot work die steel, which has the advantages that:
1. compared with the cast ingot of H13 hot work die steel prepared by the traditional vacuum melting method, the smelting method for refining inclusions in H13 hot work die steel provided by the invention has superior ingot structure and comprehensive performance, and Al in the structure2O3-SiO2The size of the inclusion-like substances is refined to be nano-scale, and the inclusion-like substances uniformly exist in the ingot in a spherical form, so that the aspect ratio of the inclusion-like substances is obviously reduced; research and analysis show that the large-size Al in the cast structure of the H13 steel prepared by the invention2O3-SiO2The amount of similar impurities is greatly reduced, and the nano-scale spherical Al2O3-SiO2The quantity and distribution of the similar inclusions are increasedMore uniform, thereby greatly prolonging the service life of the H13 hot work die steel.
2. The invention provides a smelting method for refining inclusions in H13 hot-work die steel, which adopts bottom blowing argon to generate bubbles in a melt, the bubbles flow back and forth in molten steel to form a flow field, the flow field strength in the molten steel can be adjusted by controlling the gas inlet amount to achieve a stirring effect, and nanoscale Al in the molten steel is enabled to be2O3-SiO2The similar inclusions are distributed more uniformly, and can also absorb the original gas in the molten steel and pull the extra-large-size inclusions in the molten steel into the top slag, thereby achieving the purpose of refining the inclusions.
3. The H13 hot work die steel production preparation method does not need to invest excessive production cost, the preparation method is simple and convenient to operate, and the H13 hot work die steel prepared by the method has small inclusion size and uniform distribution. In addition, the smelting method has wide application range, is not limited to H13 hot work die steel, is suitable for preparing steel ingots and castings of various materials, and has great development prospect.
Drawings
Other features, details and advantages of the present invention will become more fully apparent from the following detailed description of the specific embodiments of the invention when taken in conjunction with the accompanying drawings.
FIG. 1 is a drawing of a smelting apparatus for refining inclusions in H13 hot-work die steel in an example of the present invention. 1-composite powder of Al-Si powder wrapped by iron sheet; 2-magnetic field heating means; 3-a slag pool; 4-molten steel; 5-air brick; 6-argon gas inlet.
FIG. 2 is a schematic diagram of micro-feeding in a multi-spot area according to an embodiment of the present invention. 7-a crucible; 4-molten steel; 1-composite powder of Al-Si powder wrapped by iron sheet.
FIG. 3 is a schematic diagram of a composite powder body of Al-Si powder wrapped by iron sheet in an embodiment of the invention. 10-Al-Si powder composite powder; 11-iron sheet.
Detailed Description
For better understanding of the technical solutions of the present invention, the following detailed descriptions of the embodiments of the present invention are provided with reference to the accompanying drawings. It should be understood that the described embodiments are only some embodiments of the invention, and not all embodiments.
As shown in FIGS. 1 and 2, the embodiment of the invention provides refined Al in H13 hot work die steel2O3-SiO2The smelting method of the similar inclusion is suitable for the smelting process of H13 hot work die steel, and effectively reduces large-size Al inside the cast ingot2O3-SiO2The quantity of the impurities improves the purity of the molten steel 4 in the crucible 7. According to the kinetic and thermodynamic theory of the growth of impurities in the solidification process, the reduction of Al in steel is realized by adopting the primary smelting process of an electric arc furnace and the external refining smelting process, and feeding the composite powder 1 of the Al-Si powder wrapped by the iron sheet with the diameter of 1mm in a multi-point area micro-supply mode2O3-SiO2The size of inclusions and the reduction of the local oxygen concentration in the steel. As shown in fig. 3, the Al-Si powder-coated composite powder 1 includes an iron sheet 11 and an Al-Si powder composite powder.
The steel-making production process comprises the following steps: primary smelting in an electric arc furnace, refining in an LF furnace, feeding aluminum wires, VD vacuum refining, bottom argon blowing and casting. Selecting chemical materials according to the weight percentage of preset chemical components. The preset chemical components in percentage by weight are as follows: 0.36 wt.% of C, 1.03 wt.% of Si, Mn: 0.45 wt.%, P.ltoreq.0.002 wt.%, S.ltoreq.0.007 wt.%, V: 1.01 wt.%, Cr:4.88 wt.%, Mo: 1.31 wt.%, the balance being Fe. In the process, a specially-assigned person carries out batching, the charging amount of the furnace charge is 20t, and the charging amount of the pig iron is 18 t. In particular, when charging, a protective measure of steel plate laying or chip laying is needed for protecting the furnace bottom, and when no metal residue exists in the furnace, part of light scrap steel or chip is firstly charged to protect the furnace bottom, and then heavier scrap steel is charged into the furnace. The discharge of the materials is carried out according to the principle that the middle is high, the periphery is low, the upper part is loose and the lower part is compact.
And starting the electric arc furnace, transmitting power, and heating by the magnetic field heating device 2, wherein the smelting process comprises melting, oxidation, tapping and deoxidation alloying. Adding iron oxide white skin and lime by 3-5 batches in the melting stage before the first feeding, wherein the weight of each iron oxide white skin and lime is about 0.4 t; in the initial stage of melting, when the furnace door turns red, an oxygen lance of the furnace door is started to blow oxygen, and the oxygen is gradually adjusted from low oxygen to high oxygen. Controlling the temperature of a molten pool after melting down to be about 1550 ℃, starting to sample and analyze the element content in the steel and reduce the voltage level, and when the concentration of P does not meet the process requirement, continuously adding iron oxide white skin and lime into the furnace and controlling the temperature to further remove P. And in the melting process, oxygen, lime and iron scale are used for controlling the fluidity of the slag. In the oxidation process, the oxygen lance is opened in sequence from low oxygen to medium oxygen and then to high oxygen according to the oxygen flow control, the time interval between each grade is 2-3 minutes, the oxygen blowing time is 10-15 minutes, and steel can be tapped after the temperature of molten steel, the C content and the P content meet the technological requirements. Before tapping, an overhead bunker is adopted to add 80-160kg of lime and 4-12kg of carbon powder into a molten pool for pre-deoxidation and slag-discharging operation, and then tapping can be carried out. The slag and molten steel 4 in the slag pool 3 before tapping are required to have S less than or equal to 0.007 percent, P less than or equal to 0.002 percent and molten steel temperature more than or equal to 1680 ℃. And in the tapping process, adding a deoxidizer according to the operation requirement.
And then LF refining treatment is carried out, argon is introduced through an argon introducing port 6 below the air brick 5, after the flow of the argon introduced into the cabin body is set, oxygen measurement and sampling operations are carried out, and the free oxygen concentration is 30-100 ppm. When the temperature of the melt is more than or equal to 1600 ℃, vacuum deoxidization is directly carried out. If the temperature is less than 1600 ℃, adding 120kg of refining slag and a proper amount of lime to rapidly form slag, and heating to 1630 ℃ for vacuum deoxygenation.
And after the refining is finished, wire feeding treatment is carried out, and the used wire is composite powder 1 prepared by wrapping Al-Si powder with iron sheet 11 with the thickness of 0.1 mm. The wire feeding speed is 3-4mm/s, and the wire feeding depth is 300 mm. Ensuring that the state of the machine meets the requirements before feeding wires, and feeding wires to a plurality of areas simultaneously after slag can be broken if the slag surface is crusted; and (3) starting a bottom argon blowing device at the same time of wire feeding, and introducing argon into the melt to form a flow field in the melt. And measuring the oxygen concentration after the wire feeding is finished, and carrying out VD refining operation after the oxygen concentration reaches the standard.
Casting molten steel into a casting mold to solidify to obtain H13 hot-work mold steel cast ingot with uniform structure and excellent performance, and after subsequent rolling and heat treatment, the tensile strength is more than or equal to 1760Mpa, and the impact energy of a room-temperature V-notch impact test is more than or equal to 14.7J/cm2Meets the requirements of the North America NADCA die-casting association on high-grade high-quality H13 hot-working dieHas the performance requirement of steel.
Claims (5)
1. A smelting method for refining inclusions in H13 hot-work die steel is characterized in that in the smelting process, a multipoint regional micro-supply method is adopted to feed composite powder of Al-Si powder wrapped by iron sheet into molten steel, and the composite powder is combined with oxygen in the molten steel to form a large amount of nano-scale Al2O3-SiO2An inclusion; and in the smelting process, a bottom blowing argon mode is adopted, the grade of the inclusions A + B + C + D + DS is less than or equal to 2.5, and finally the high-grade high-quality H13 hot-work die steel cast ingot is obtained.
2. The method for smelting refined inclusions in H13 hot work die steel as claimed in claim 1, wherein the method comprises the steps of:
step 1: configuring chemical materials according to the preset weight percentage of the element components of the H13 hot work die steel, wherein the chemical materials are placed according to the material placing principle that the middle of a material placing region is high, the periphery of the material placing region is low, the lower half part is used for placing materials compactly, and the upper half part is used for placing materials loosely;
step 2: preparing H13 hot die steel liquid and alloying by adopting a smelting mode of smelting and heating in a vacuum arc furnace;
and step 3: after alloying operation, feeding the composite powder of Al-Si powder wrapped by iron sheet into molten steel in a multipoint regional micro-supply mode;
and 4, step 4: feeding powder into the melt, then measuring the oxygen concentration, and carrying out VD vacuum refining operation when the concentration of free oxygen is about 10 ppm;
and 5: forming a flow field in the melt by bottom blowing argon into the melt, so that powder wrapped in the molten iron sheet is uniformly distributed in the molten steel;
step 6: and pouring the prepared H13 hot-work die steel liquid into a casting mold to be uniformly solidified, and analyzing the size, the form, the components, the quantity and the distribution of inclusions in the ingot casting structure.
3. The smelting method for refining inclusions in H13 hot-work die steel as claimed in claim 1, wherein the hot-work die steel comprises the following chemical components in percentage by weight: 0.32-0.45 wt.% of C, 0.80-1.20 wt.% of Si, 0.20-0.50 wt.% of Mn, 0.80-1.20 wt.% of V, 4.75-5.50 wt.% of Cr, 1.10-1.75 wt.% of Mo, less than or equal to 0.03 wt.% of P, less than or equal to 0.03 wt.% of S, and the balance of Fe.
4. The method for smelting refined inclusions in H13 hot-work die steel as claimed in claim 2, wherein the smelting mode of vacuum arc furnace smelting heating in step 2 is characterized in that before tapping, a high-level bunker is used to add 400kg lime and 10-30kg carbon powder into a molten pool for pre-deoxidation and slag tapping after the operation is finished; in the step 2, the smelting mode of the vacuum arc furnace for smelting and heating, the preparation of molten steel and the alloying operation comprise: and heating and melting the alloy into molten steel by using a vacuum melting heating mode, carrying out alloying operation after the molten steel is completely melted, and then overheating and heating to 50-100 ℃ until the molten steel surface is stable.
5. The method for smelting refined inclusions in H13 hot-work die steel as claimed in claim 2, wherein the Al-Si powder-coated composite powder in step 3 is fed into the molten steel in a multipoint region micro-feeding mode, and the powder feeding depth is more than 300 mm; the thickness of the iron sheet is 0.1-0.2 mm, and the melting time of the iron sheet is 1-1.5 s.
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